D-赖氨酸盐酸盐的制备研究

Preparation of D-lysine monohydrochloride from L-lysine monohydrochloride

目的:从L-赖氨酸盐酸盐制备D-赖氨酸盐酸盐。方法:经L-赖氨酸盐酸盐消旋制得的DL-赖氨酸,以L-酒石酸为手性拆分剂,生成D-赖氨酸-L-酒石酸盐,再经无机酸钙沉淀L-酒石酸,制得D-赖氨酸盐酸盐。结果:DL-赖氨酸与L-酒石酸反应适宜的摩尔比为1∶0.8,反应温度为60～70℃。碳酸钙、氢氧化钙和氧化钙分离D-赖氨酸的收率分别为34.6%,34.0%和33.9%,含量分别为85.7%,90.3%和90.6%。纯化后的D-赖氨酸盐酸盐产品,其含量和光学纯度均达99%以上。结论:用L-酒石酸拆分DL-赖氨酸是可行的,用无机酸钙分离D-赖氨酸与L-酒石酸是有效的。

Objective： To prepare D-lysine monohydrochloride from L-lysine monohydrochloride. Meth- ods： After racemization of L-lysine monohydrochloride, the obtained DL-lysine was resoluted to D-lysine-L-tartrate using L-tartaric acid as resolving agent; subsequently D-lysine monohydrochloride was separated from calcium tar- trate precipitation by inorganic acid calcium. Results ： The optimum conditions of resolution reaction involved 1 ： 0.8 molar ratio of DL-lysine to L-tartaric acid at 60 70 C reaction temperature. The yields of crude D-lysine from D- lysine-L-tartrate solution after precipitation using calcium carbonate, calcium hydroxide and calcium oxide were 34.6% , 34.0% and 33.9% with purities of 85.7% , 90.3% and 90.6% , respectively. Both the chemical purity and optical purity of the purified D-lysine monohydrochloride were above 99%. Conclusion： The resolution of DL- lysine using L-tartaric acid as resolving agent is teasible, and the separation of D-lysine from D-lysine-L-tartrate is effective with inorganic acid calcium.